CN114210982B - Method for preparing Cu-Cr2Nb alloy with nano structure - Google Patents
Method for preparing Cu-Cr2Nb alloy with nano structure Download PDFInfo
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Abstract
The invention discloses a method for preparing Cu-Cr with nano structure by adopting a pure copper ball milling tank and ball milling balls 2 A method of Nb alloy comprising the steps of: s1, preparing nano Cr 2 Nb powder, S2, preparation of composite Cu-Cr 2 Nb powder, S3, hot-pressing sintering. The invention adopts a pure copper ball milling tank and a pure copper ball milling ball pair Cr 2 Nb powder and Cu-Cr 2 The Nb powder is subjected to high-energy ball milling, so that the powder is refined, fine and nanoscale powder can be obtained, and impurities are not brought in. The hot-pressed sintering is carried out in a pure hydrogen environment or a hydrogen mixing environment, so that the compact Cu-Cr with high strength and nano structure can be obtained 2 The Nb alloy has very low oxygen content, excellent heat conducting performance and high temperature performance, and long service life.
Description
Technical Field
The invention relates to the technical field of alloy material preparation, in particular to a method for preparing a Cu-Cr2Nb alloy with a nano structure by adopting a pure copper ball milling tank and ball milling balls.
Background
Cu-Cr 2 Nb alloys are a series of different Cr 2 Examples of the Cu alloy containing Nb include Cu-8Cr-4Nb (at.%), cu-4Cr-2Nb (at.%), cu-2Cr-1Nb (at.%), etc. Cu-8Cr-4Nb (at.%) alloy, GRCop-84 alloy (Glenn Research Copper alloy 84), was developed by the American Greennel research center and used mainly as a lining material for rocket main engines combustors and nuclear reactors, and GRCop-84 alloy was usedThe performance of rocket engines and nuclear reactors can be significantly improved.
Cu-Cr 2 Nb alloys have excellent thermal conductivity. While when Cu-Cr 2 When the Nb alloy contains a component having a low heat conductive property, cu-Cr 2 The thermal conductivity of Nb alloy will be significantly reduced. For example, when Cu-Cr 2 Nb alloy contains Fe and SiO with lower heat conduction performance 2 Cu-Cr in the case of 2 The heat conducting property of the Nb alloy is reduced; fe. SiO (SiO) 2 The higher the content, the lower the heat conducting properties of the alloy.
Cu-Cr 2 The Nb alloy has good high-temperature performance. Cu-Cr 2 Nb is a dispersion-strengthened Cu alloy with a strengthening phase of alpha Cr 2 Nb (Laves phase) is an intermetallic compound. Strengthening phase alpha Cr 2 The finer the Nb, the Cu-Cr 2 The better the high temperature properties of the Nb alloy.
High-energy ball milling is a mature fine powder technology. As the materials of the common ball-milling tank and ball-milling balls are mainly stainless steel materials, some ball-milling tanks and balls are agates (the main component is SiO 2 ). Therefore, after high-energy ball milling, the powder inevitably contains iron and SiO 2 Finally result in Cu-Cr 2 The heat conducting property of the Nb alloy is obviously reduced. That is why common ball-milling pot and ball pairs of Cu-Cr cannot be used 2 The main reason for high-energy ball milling of Nb alloy powder.
Disclosure of Invention
Aiming at the problems pointed out by the background technology, the invention provides a method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting a pure copper ball milling tank and ball milling balls.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 5-20: 1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is in a micron order;
s1-3, sealing and ball milling:
sealing the pure copper ball milling tank, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling to obtain nano Cr2Nb powder;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
Mixing the nano Cr2Nb powder prepared in the step S1-3 with a certain amount of copper powder; placing the mixed powder and a certain amount of pure copper ball milling balls into another pure copper ball milling tank, wherein the ball-to-material ratio is 5-20: 1, a step of;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling to obtain composite Cu-Cr2Nb powder with a nano structure;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing sintering, cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure.
Further, in the above scheme, the diameter of the pure copper ball mill ball in the step S1-1 is 2-20 mm.
Pure copper ball grinding ball and Cr 2 In the high-energy ball milling process of Nb powder in a pure copper ball milling tank, cr is used for 2 Nb powder has high hardness, high brittleness, low pure copper hardness and good toughness, so Cr is used in high-energy ball milling 2 Part of Cr in the process of crushing Nb powder under impact 2 Nb particles will inevitably be embedded into the surface of the pure copper ball milling pot and the pure copper ball milling balls, which will facilitate the subsequent Cr 2 The Nb powder is continuously crushed, and the pure copper ball milling tank and the pure copper ball milling balls can be used for a plurality of timesFor Cr 2 Refining Nb powder.
Further, in the above scheme, the particle size of the Cr2Nb powder in the step S1-2 is 100-1000 μm.
Further, in the above scheme, the weight ratio of the nano Cr2Nb powder to the copper powder in step S2-1 is 1:2 to 60. The content of Cr2Nb has a great influence on the performance of Cu-Cr2Nb alloy. However, when the weight ratio of Cr2Nb to copper powder is greater than 1:2, the alloy has no use value; when the weight ratio of Cr2Nb to copper powder is less than 1:60, at this time, the content of Cr2Nb has less influence on the performance of the Cu-Cr2Nb alloy. Therefore, the weight ratio of Cr2Nb powder to copper powder is set to be 1:2 to 60.
Further, in the above scheme, the high-energy ball milling time in the step S1-3 and the step S2-2 is 0.5-20 hours, and the rotational speed of the high-energy ball milling is 100-1000 rpm. The time and the rotating speed of the high-energy ball milling have great influence on the size and the particle size distribution of the ball milling powder. When the time of high-energy ball milling is less than 0.5 hour or the rotating speed of high-energy ball milling is less than 100 revolutions per minute, the influence of the time and the rotating speed of the high-energy ball milling on the size and the particle size distribution of the ball milling powder is small; when the time of high-energy ball milling is more than 20 hours or the rotational speed of high-energy ball milling is more than 1000 rpm, the fine ball mill may be re-polymerized together due to too large surface energy of cold welding or fine powder. Therefore, the invention sets the time of high-energy ball milling to 0.5-20 hours and the rotating speed of high-energy ball milling to 100-1000 rpm.
Nano Cr 2 In the process of performing high-energy ball milling on Nb powder and copper powder in a pure copper ball milling tank, cr is used as a raw material 2 High Nb hardness, high brittleness, low pure copper hardness and good toughness, thus, part of Cr 2 Nb particles will inevitably be embedded in the surface of the pure copper ball mill pot and pure copper balls, which will result in Cr in the ball mill pot when the pure copper ball mill pot is first used 2 The quality of Nb powder is reduced. But with Cr 2 Nb particles are embedded into the surfaces of the pure copper ball milling tank and the pure copper balls to achieve dynamic balance, cr 2 The case of Nb mass reduction will substantially disappear. The ball milling tank and the ball milling ball are convenient for multiple times of Cu-Cr preparation of nano structures 2 Nb powder.
Further, in the above scheme, in the step S3, the hot pressing furnace is in a pure hydrogen environment or a mixed hydrogen environment. The pure hydrogen environment or the mixed hydrogen environment is used for keeping the hot pressing furnace in a reducing atmosphere, and the hot pressing furnace have no difference in function.
Further, in the above scheme, the hydrogen mixing environment is a mixed gas of hydrogen and nitrogen, or a mixed gas of hydrogen and argon.
Further, in the above scheme, the hydrogen content in the hydrogen mixing environment is 5-100% by volume.
Hot pressed sintering in pure hydrogen environment or mixed hydrogen environment can obtain compact, high strength and nanometer structure Cu-Cr 2 Nb alloys, and the oxygen content of the alloy will be very low.
Further, in the above scheme, the hot pressing pressure of the hot pressing sintering in the step S3 is 5-50 Mpa, the sintering temperature is 850-1100 ℃, the hot pressing pressure is 5-50 Mpa, and the heat preservation time is 0.5-3.0 hours. As the hot pressing pressure has a larger influence on the compactness of the Cu-Cr2Nb alloy, the higher the hot pressing pressure is, the higher the compactness is. In addition, graphite materials (the compression limit of graphite is 60 Mpa) are commonly adopted in the hot-pressing die at present, so that the hot-pressing pressure of the invention is set to be 5-50 Mpa in order to ensure sintering densification and repeated use of the graphite die. Because the sintering temperature has a great influence on the compactness of the Cu-Cr2Nb alloy, when the sintering temperature is lower than 850 ℃, the alloy cannot be sintered compactly; when the sintering temperature is higher than 1100 ℃, the alloy is melted and cannot be sintered and formed, so the sintering temperature of the invention is set to 850-1100 ℃. The heat preservation time has a great influence on the compactness and alloying of the Cu-Cr2Nb alloy. When the heat preservation time is less than 0.5 hour, the Cu-Cr2Nb alloy has lower density and lower alloying degree; when the heat preservation time is higher than 3.0 hours, the influence of the heat preservation time on the density and alloying degree of the Cu-Cr2Nb alloy is small, and only waste is formed when the heat preservation time is continuously increased, so that the sintering time is set to be 0.5-3.0 hours.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the Cr2Nb powder and the Cu-Cr2Nb powder are subjected to high-energy ball milling by adopting a pure copper ball milling tank and pure copper ball milling balls, so that the powder is refined, fine and nano-grade powder can be obtained, and impurities are not brought in.
Secondly, hot-pressed sintering is carried out in a pure hydrogen environment or a hydrogen mixing environment, so that compact, high-strength and nano-structured Cu-Cr can be obtained 2 Nb alloys, and the oxygen content of the alloy will be very low.
Third, the nanostructured Cu-Cr prepared by the method of the present invention 2 Nb alloy, and existing Cu-Cr 2 Nb alloys have many advantages: (1) Strengthening phase Cr in alloy 2 Nb is very fine, some Cr 2 Nb particles reach the nanometer level; (2) Strengthening phase Cr in alloy 2 Nb is dispersed and distributed very uniformly; (3) Cu-Cr with nanostructure 2 The impurity content in the Nb alloy is very low, fe is completely absent, and the O content is very low; (4) Cu-Cr with nanostructure 2 The Nb alloy has excellent heat conducting performance and high temperature performance, and the service life of the alloy can be obviously prolonged.
Drawings
FIG. 1 is a diagram of the gold phase of Cr2Nb powder ball-milled to submicron order with high energy prepared in example 2 of the present invention.
Description of the embodiments
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameters of 2-3 mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 5:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 100-150 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 0.5 hour, and the rotating speed is 100 rpm, so that nano Cr2Nb powder can be obtained;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:2 weight ratio; the mass ratio corresponds to Cu-28Cr-14Nb (at.%); mixing the powder and pure copper ball mill balls according to a ratio of 5:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 0.5 hour, and the rotating speed is 100 revolutions per minute, so that the composite Cu-Cr2Nb powder with the nano structure can be obtained;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is in a pure hydrogen environment, the hot pressing pressure of hot pressing and sintering is 5Mpa, the sintering temperature is 850 ℃, and the heat preservation time is 0.5 hour. And cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure.
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameter of 10-12 mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 18:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 500-600 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 15 hours, and the rotating speed is 600 revolutions per minute, so that nano Cr2Nb powder can be obtained;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:10 weight ratio; the mass ratio corresponds to Cu-6Cr-3Nb (at.%); mixing the powder with pure copper ball milling balls according to the following ratio of 18:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 10 hours, and the rotating speed is 600 revolutions per minute, so that the composite Cu-Cr2Nb powder with the nano structure can be obtained;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is filled with hydrogen and nitrogen, and the hydrogen content is 50% by volume. The hot pressing pressure of hot pressing sintering is 15Mpa, the sintering temperature is 950 ℃, and the heat preservation time is 2.0 hours. And cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure.
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameters of 18-20 mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 20:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 900-1000 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 20 hours, and the rotating speed is 1000 rpm, so that nano Cr2Nb powder can be obtained;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:30 weight ratio; the mass ratio corresponds to Cu-2Cr-1Nb (at.%) alloy; mixing the powder with pure copper ball milling balls according to the following ratio of 20:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 20 hours, and the rotating speed is 1000 revolutions per minute, so that the composite Cu-Cr2Nb powder with the nano structure can be obtained;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is filled with hydrogen and argon, and the hydrogen content is 90% by volume. The hot pressing pressure of hot pressing sintering is 30Mpa, the sintering temperature is 1100 ℃, and the heat preservation time is 3.0 hours. And cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure.
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameter of 10mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 10:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 200-300 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 5 hours, the rotating speed is 500 rpm, the machine is stopped for 0.5 hour after the operation is carried out for 0.5 hour, radiating, and opening the ball milling tank after the ball milling is finished, and taking out fine and nano Cr2Nb powder;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:7, which corresponds to a Cu-8Cr-4Nb (at.%) alloy; mixing the powder and pure copper ball mill balls according to the following ratio of 10:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 5 hours, the rotating speed is 500 revolutions per minute, and the pure copper ball milling tank is stopped for 0.5 hour after 0.5 hour for heat dissipation; after the ball milling is completed, due to Cr 2 Nb mass is reduced and therefore this ball mill is discarded;
repeating the step S2-1 and the step S2-2 to obtain the composite Cu-Cr2Nb powder with the nano structure;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; putting a die filled with Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is filled with hydrogen and nitrogen, and the hydrogen content is 5% by volume; the hot pressing pressure of hot pressing sintering is 3Mpa, the sintering temperature is 900 ℃, the heat preservation time is 2.0 hours, the alloy is taken out after cooling, and finally the Cu-8Cr-4Nb (at%) alloy with the nano structure is obtained.
Strengthening phase Cr in the nano-structured Cu-8Cr-4Nb (at.%) alloy prepared in the example 2 Nb is very fine and most of Cr 2 Nb particles less than 100 nm; strengthening phase Cr in alloy 2 Nb is dispersed and distributed very uniformly; the Cu-8Cr-4Nb (at%) alloy with nano structure has very low impurity content, no Fe content, very low O content and less than 20ppm; the Cu-8Cr-4Nb (at%) alloy with the nano structure has excellent heat conduction performance and high temperature performance, compared with the existing Cu-8Cr-4Nb (at%) alloy, the heat conduction coefficient is increased by more than 10%, the yield strength is increased by more than 15%, and the service life of the alloy can be obviously prolonged by more than 10%.
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameters of 13-16 mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 17:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 700-900 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 17 hours, and the rotating speed is 900 revolutions per minute, so that nano Cr2Nb powder can be obtained;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:60 weight ratio; the mass ratio corresponds to Cu-1Cr-0.5Nb (at.%) alloy; mixing the powder with pure copper ball milling balls according to the following ratio of 17:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 20 hours, and the rotating speed is 1000 revolutions per minute, so that the composite Cu-Cr2Nb powder with the nano structure can be obtained;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is filled with hydrogen and argon, and the hydrogen content is 75% by volume. The hot pressing pressure of hot pressing sintering is 35Mpa, the sintering temperature is 1070 ℃, and the heat preservation time is 2.8 hours. And cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure.
Strengthening phase Cr in the nano-structured Cu-Cr2Nb (at.%) alloy prepared in the example 2 Nb is very fine and most of Cr 2 Nb particles less than 100 nm; strengthening phase Cr in alloy 2 Nb is dispersed and distributed very uniformly; the Cu-Cr2Nb (at%) alloy with the nano structure has very low impurity content, no Fe, and very low O content of less than 20ppm; the Cu-Cr2Nb (at%) alloy with the nano structure has excellent heat conduction performance and high temperature performance, compared with the existing Cu-Cr2Nb (at%) alloy, the heat conduction coefficient is increased by more than 10%, the yield strength is increased by more than 15%, and the service life of the alloy can be obviously prolonged by more than 10%.
Examples
The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls comprises the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls with the diameter of 12mm are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 15:1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is 700-800 mu m;
s1-3, sealing and ball milling:
sealing a pure copper ball milling tank, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 7 hours, the rotating speed is 700 rpm, the machine is stopped for 0.5 hour after the operation is performed for 0.5 hour for heat dissipation, and after the ball milling is completed, opening the ball milling tank, and taking out fine and nano Cr2Nb powder;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
The nano Cr2Nb powder prepared in the step S1-3 and copper powder are mixed according to the following ratio of 1:15.3, which corresponds to a Cu-4Cr-2Nb (at.%); mixing the powder with pure copper ball milling balls according to the following ratio of 15:1 ball material ratio is put into another pure copper ball milling tank;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, putting the sealed pure copper ball milling tank on a ball mill for high-energy ball milling, wherein the ball milling time is 7 hours, the rotating speed is 700 rpm, the rotating speed is 500 rpm, and the machine is stopped for 0.5 hour after 0.5 hour for heat dissipation; after the ball milling is completed, due to Cr 2 Nb mass is reduced and therefore this ball mill is discarded;
repeating the step S2-1 and the step S2-2 to obtain the composite Cu-Cr2Nb powder with the nano structure;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; and (3) putting the die filled with the Cu-Cr2Nb powder into a hot pressing furnace for hot pressing and sintering, wherein the hot pressing furnace is filled with hydrogen and argon, the hydrogen content is 10% by volume in a hydrogen mixing environment, the hot pressing pressure of hot pressing and sintering is 5Mpa, the sintering temperature is 930 ℃, and the heat preservation time is 1.5 hours. And cooling and taking out to finally obtain the Cu-4Cr-2Nb (at%) alloy with the nano structure.
The strengthening phase Cr2Nb in the nano-structured Cu-4Cr-2Nb (at.%) alloy prepared by the embodiment is very fine, and most Cr2Nb particles are smaller than 100 nm; the strengthening phase Cr2Nb in the alloy is dispersed and distributed very uniformly; the Cu-4Cr-2Nb (at%) alloy with nano structure has very low impurity content, no Fe content, very low O content and less than 20ppm; the Cu-4Cr-2Nb (at%) alloy with the nano structure has excellent heat conduction performance and high temperature performance, and compared with the existing Cu-4Cr-2Nb (at%) alloy, the heat conduction coefficient is increased by more than 15%, the yield strength is increased by more than 15%, and the service life of the alloy can be obviously prolonged by more than 15%.
Claims (6)
1. The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls is characterized by comprising the following steps:
s1, preparing nano Cr2Nb powder
S1-1, preparing a pure copper ball milling tank and pure copper ball milling balls:
machining two pure copper ball milling tanks with the same size according to the size of a steel ball milling tank configured by a ball mill, wherein one pure copper ball milling tank is used for ball milling Cr2Nb powder, the other pure copper ball milling tank is used for ball milling Cu powder and Cr2Nb powder, and a plurality of pure copper ball milling balls are prepared;
s1-2, ball milling preparation:
according to the ball-material ratio of 5-20: 1, weighing pure copper ball milling balls and Cr2Nb powder, and putting the pure copper ball milling balls and the Cr2Nb powder into a pure copper ball milling tank prepared in the step S1, wherein the particle size of the Cr2Nb powder is in a micron order;
s1-3, sealing and ball milling:
sealing the pure copper ball milling tank, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling to obtain nano Cr2Nb powder;
s2, preparing composite Cu-Cr 2 Nb powder:
s2-1: mixing material
Mixing the nano Cr2Nb powder prepared in the step S1-3 with a certain amount of copper powder; placing the mixed powder and a certain amount of pure copper ball milling balls into another pure copper ball milling tank, wherein the ball-to-material ratio is 5-20: 1, a step of;
s2-2, ball milling:
sealing the pure copper ball milling tank in the step S2-1, and then placing the sealed pure copper ball milling tank on a ball mill for high-energy ball milling to obtain composite Cu-Cr2Nb powder with a nano structure;
s3, hot-pressing sintering:
putting the composite Cu-Cr2Nb powder with the nano structure prepared in the step S2-2 into a mold for molding; putting a die filled with Cu-Cr2Nb powder into a hot pressing furnace for hot pressing sintering, cooling and taking out to finally obtain the Cu-Cr2Nb alloy with the nano structure;
the high-energy ball milling time of the step S1-3 and the step S2-2 is 0.5-20 hours, and the rotating speed of the high-energy ball milling is 100-1000 rpm;
s3, the hot pressing furnace is in a pure hydrogen environment or a hydrogen mixing environment;
the hydrogen mixing environment is a mixed gas of hydrogen and nitrogen or a mixed gas of hydrogen and argon.
2. The method for preparing the nano-structured Cu-Cr2Nb alloy by adopting the pure copper ball milling tank and the ball milling balls, which is disclosed in the claim 1, is characterized in that the diameter of the pure copper ball milling balls in the step S1-1 is 2-20 mm.
3. The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls, which is characterized in that the grain size of the Cr2Nb powder in the step S1-2 is 100-1000 mu m.
4. The method for preparing the nano-structured Cu-Cr2Nb alloy by adopting the pure copper ball milling tank and the ball milling balls as claimed in claim 1, wherein the weight ratio of the nano Cr2Nb powder to the copper powder in the step S2-1 is 1:2 to 60.
5. The method for preparing the Cu-Cr2Nb alloy with the nano structure by adopting the pure copper ball milling tank and the ball milling balls, which is disclosed in claim 1, is characterized in that the hydrogen content in the hydrogen mixing environment is 5-100% by volume.
6. The method for preparing the nano-structured Cu-Cr2Nb alloy by adopting the pure copper ball milling tank and the ball milling balls, which is characterized in that the hot press sintering in the step S3 has the hot press pressure of 5-50 Mpa, the sintering temperature of 850-1100 ℃, the hot press pressure of 5-50 Mpa and the heat preservation time of 0.5-3.0 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701300A (en) * | 2009-11-11 | 2010-05-05 | 昆明理工大学 | Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method |
| CN106148756A (en) * | 2016-08-17 | 2016-11-23 | 中国科学院长春应用化学研究所 | The preparation method of one Albatra metal |
| CN108085534A (en) * | 2017-12-21 | 2018-05-29 | 湖北工业大学 | A kind of in-situ synthesis of boride titanium enhancing Cu-base composites and its preparation method and application |
| CN109022895A (en) * | 2018-08-28 | 2018-12-18 | 河南科技大学 | A kind of preparation method of the high-densit high copper content Cu-W alloy of Ultra-fine Grained |
| JP2021031691A (en) * | 2019-08-19 | 2021-03-01 | 山陽特殊製鋼株式会社 | Cu alloy powder |
-
2021
- 2021-11-16 CN CN202111357438.1A patent/CN114210982B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701300A (en) * | 2009-11-11 | 2010-05-05 | 昆明理工大学 | Method for preparing titanium diboride dispersion-strengthened Cu-base composites by using mechanical alloying method |
| CN106148756A (en) * | 2016-08-17 | 2016-11-23 | 中国科学院长春应用化学研究所 | The preparation method of one Albatra metal |
| CN108085534A (en) * | 2017-12-21 | 2018-05-29 | 湖北工业大学 | A kind of in-situ synthesis of boride titanium enhancing Cu-base composites and its preparation method and application |
| CN109022895A (en) * | 2018-08-28 | 2018-12-18 | 河南科技大学 | A kind of preparation method of the high-densit high copper content Cu-W alloy of Ultra-fine Grained |
| JP2021031691A (en) * | 2019-08-19 | 2021-03-01 | 山陽特殊製鋼株式会社 | Cu alloy powder |
Non-Patent Citations (2)
| Title |
|---|
| 王聪利 ; 张航 ; 吴斌 ; 庾高峰 ; .微量Mn对Cu-Ni-Si合金性能组织的影响.科技致富向导.2014,(第24期),全文. * |
| 黄铭刚 ; 鲁世强 ; 肖璇 ; 胡平 ; 李鑫 ; .球磨时间对软第二相韧化Cr_2Nb基复合材料组织与性能的影响.热加工工艺.2008,(第16期),全文. * |
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Application publication date: 20220322 Assignee: SIRUI ADVANCED COPPER ALLOY Co.,Ltd. Assignor: SHAANXI SIRUI ADVANCED MATERIALS Co.,Ltd. Contract record no.: X2023980040047 Denomination of invention: A Method for Preparing Nanostructured Cu Cr2Nb Alloy Granted publication date: 20230512 License type: Common License Record date: 20230821 |
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